Agilent Technologies G7035A Manuel utilisateur

Agilent Technologies

Agilent 5977 Series

MSD

Operation Manual

2 5977 Series MSD Operation Manual

Notices

No part of this manual may be reproduced in

any form or by any means (including elec-

tronic storage and retrieval or translation

into a foreign language) without prior agree-

ment and written consent from Agilent

Technologies, Inc. as governed by United

States and international copyright laws.

Manual Part Number

G3870-90003

Edition

First edition, February 2013

Printed in USA

Agilent Technologies, Inc.

5301 Stevens Creek Boulevard

Santa Clara, CA 95051

Warranty

The material contained in this docu-

ment is provided “as is,” and is sub-

ject to being changed, without notice,

in future editions. Further, to the max-

imum extent permitted by applicable

law, Agilent disclaims all warranties,

either express or implied, with regard

to this manual and any information

contained herein, including but not

limited to the implied warranties of

merchantability and fitness for a par-

ticular purpose. Agilent shall not be

liable for errors or for incidental or

consequential damages in connec-

tion with the furnishing, use, or per-

formance of this document or of any

information contained herein. Should

Agilent and the user have a separate

written agreement with warranty

terms covering the material in this

document that conflict with these

terms, the warranty terms in the sep-

arate agreement shall control.

Safety Notices

CAUTION

A CAUTION notice denotes a

hazard. It calls attention to an

operating procedure, practice, or

the like that, if not correctly

performed or adhered to, could

result in damage to the product or

loss of important data. Do not

proceed beyond a CAUTION notice

until the indicated conditions are

fully understood and met.

WARNING

A WARNING notice denotes a

hazard. It calls attention to an

operating procedure, practice, or

the like that, if not correctly

performed or adhered to, could

result in personal injury or death.

Do not proceed beyond a

WARNING notice until the

indicated conditions are fully

understood and met.

Agilent 5977 Series 3

About This Manual

This manual contains information for operating and

maintaining the Agilent 5977 Series Mass Selective Detector

(MSD) systems.

1 “Introduction”

Chapter 1 describes general information about the 5977 Series

MSDs, including a hardware description, general safety

warnings, and hydrogen safety information.

2 “Installing GC Columns”

Chapter 2 shows you how to prepare a capillary column for use

with the MSD, install it in the GC oven, and connect it to the

MSD using the GC/MSD interface.

3 “Operating in Electron Ionization (EI) Mode”

Chapter 3 describes basic tasks such as setting temperatures,

monitoring pressures, tuning, venting, and pumpdown. Much of

the information in this chapter also applies to CI operation.

4 “Operating in Chemical Ionization (CI) Mode”

Chapter 4 describes additional tasks necessary to operate in CI

mode.

5 “General Maintenance”

Chapter 5 describes maintenance procedures common to both

EI and CI instruments.

6 “CI Maintenance”

Chapter 6 describes maintenance procedures unique to CI

MSDs.

4 5977 Series MSD Operation Manual

Online User Information

Now your Agilent instrument documentation is in one place, at

your fingertips.

The software DVD that ships with your instrument provides an

extensive collection of online help, videos, and books for the

Agilent 7890 Series GC, 7820 GC,5977 Series MSD, and the 7693A.

Included are localized versions of the information you need

most, such as:

• Getting Familiar documentation

• Safety and Regulatory guides

• Installation information

• Operating guides

• Maintenance information

• Troubleshooting details

5977 Series MSD Operation Manual 5

Contents

1 Introduction

5977 Series MSD Version 10

Abbreviations Used 11

The 5977 Series MSD 13

MSD Hardware Description 15

Important Safety Warnings 17

Hydrogen Safety 19

GC precautions 19

Precautions 22

Safety and Regulatory Certifications 24

Cleaning/Recycling the Product 27

Liquid Spillage 27

Moving or Storing the MSD 27

To Replace the Primary Fuses 28

2 Installing GC Columns

Columns 32

To Install a Capillary Column in a Split/Splitless Inlet 34

To Condition a Capillary Column 37

To Install a Capillary Column in the GC/MS Interface 38

To Prepare the Column Ends for a CFT Fitting 41

3 Operating in Electron Ionization (EI) Mode

Operating the MSD from the Data System 46

Operating the MSD from the LCP 46

Modes of operation 46

6 5977 Series MSD Operation Manual

LCP status messages 48

To view system status during startup 49

LCP menus 50

The EI GC/MSD Interface 53

Before You Turn On the MSD 55

Pumping Down 56

Controlling Temperatures 56

Controlling Column Flow 56

Venting the MSD 57

To View MSD Temperature and Vacuum in Manual Tune 58

To Set Monitors for MSD Temperature and Vacuum Status 59

To Set Analyzer Temperatures from the Instrument Control

To Set the GC/MSD Interface Temperature from MassHunter 63

To Monitor High Vacuum Pressure 64

To Calibrate Column Flow Linear Velocity 66

To Tune the MSD in EI Mode 69

To Verify System Performance 71

To Perform High-Mass Testing (5977 Series MSDs) 72

To Open the MSD Covers 75

To Vent the MSD 76

To Open the Analyzer Chamber 78

To Close the Analyzer Chamber 80

To Pump Down the MSD in EI Mode 84

To Move or Store the MSD 86

5977 Series MSD Operation Manual 7

4 Operating in Chemical Ionization (CI) Mode

General Guidelines 90

The CI GC/MSD Interface 91

CI Autotune 93

To Operate the CI MSD 95

To Switch from the Standard or Inert EI ion source to the CI Ion

Source 96

To Switch from the Extractor EI Ion Source to the CI Ion

Source 97

To Pump Down the MSD in CI Mode 98

To Set Up the Software for CI Operation 99

To Operate the Reagent Gas Flow Control Module 101

To Set Up Methane Reagent Gas Flow 104

To Use Other Reagent Gases 106

To Switch from the CI Ion Source to the Standard or Inert EI Ion

Source 109

To Switch from the CI Ion Source to the Extractor EI Ion

Source 110

To Perform a PCI Autotune (Methane Only) 111

To Perform an NCI Autotune (Methane Reagent Gas) 113

To Verify PCI Performance 115

To Verify NCI Performance 116

To Monitor CI Mode High Vacuum Pressure 117

5 General Maintenance

Before Starting 120

Maintaining the Vacuum System 125

8 5977 Series MSD Operation Manual

Maintaining the Analyzer 126

To Remove the EI Ion Source 128

To Disassemble the Standard or Inert EI Ion Source 131

To Disassemble the Extractor EI Ion Source 134

To Clean the EI Ion Source 137

To Assemble a Standard or Inert EI Ion Source 142

To Assemble the Extractor EI Ion Source 145

To Replace a Filament in an EI Ion Source 148

To Install the EI Ion Source 150

To Replace the Electron Multiplier Horn 151

6 CI Maintenance

General Information 154

To set up your MSD for CI operation 154

To Install the CI/Extractor Interface Tip Seal 155

To Remove the CI Ion Source 157

To Disassemble the CI Ion Source 159

To Clean the CI Ion Source 162

To Assemble the CI Ion Source 164

To Install the CI Ion Source 167

To Replace a Filament in a CI Ion Source 168

Agilent 5977 Series MSD

Operation Manual

Agilent Technologies

Introduction

5977 Series MSD Version 10

Abbreviations Used 11

The 5977 Series MSD 13

MSD Hardware Description 15

Important Safety Warnings 17

Hydrogen Safety 19

Safety and Regulatory Certifications 24

Cleaning/Recycling the Product 27

Liquid Spillage 27

Moving or Storing the MSD 27

To Replace the Primary Fuses 28

This chapter describes general information about the 5977 Series MSDs,

including a hardware description, general safety warnings, and hydrogen

safety information.

10 5977 Series MSD Operation Manual

1Introduction

5977 Series MSD Version

5977 Series MSDs are equipped with a high performance turbomolecular

(turbo) pump or a diffusion pump, and a choice of three foreline pumps. In

addition, there are two types of analyzers (stainless steel or inert) and four

types of ion sources. The serial number label displays a product number

(Table 1) that indicates what type of MSD you have.

Table 1 Available high vacuum pumps

Model name Product number Description Ionization mode/Type

5977E MSD Diff Pump for 7820 GC G7035A Diffusion pump Electron ionization

(EI)/Stainless Steel

5977E MSD Turbo Pump for 7820 GC G7036A Performance Turbo pump Electron ionization

(EI)/Stainless Steel

5977A VL inert MSD

EI Diffusion Pump for 7890 Series GC

G7037A Diffusion pump MSD Electron ionization (EI) /Inert

5977A inert MSD EI Turbo for

7890 Series GC

G7038A Performance turbo pump

MSD

Electron ionization (EI) /Inert

5977A extractor MSD EI Perf Turbo

for 7890 Series GC

G7039A Performance turbo pump

MSD

Electron ionization

(EI)/Extractor

5977A EI/CI MSD for 7890 Series GC G7040A Performance turbo pump

MSD

Electron ionization

(EI) /Extractor

Chemical ionization /PCI, NCI

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